JPS6311579A - Manufacture of fiber reinforced ceramics - Google Patents
Manufacture of fiber reinforced ceramicsInfo
- Publication number
- JPS6311579A JPS6311579A JP61152891A JP15289186A JPS6311579A JP S6311579 A JPS6311579 A JP S6311579A JP 61152891 A JP61152891 A JP 61152891A JP 15289186 A JP15289186 A JP 15289186A JP S6311579 A JPS6311579 A JP S6311579A
- Authority
- JP
- Japan
- Prior art keywords
- reinforcing fibers
- surfactant
- mixed
- water
- organic solvent
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 239000011226 reinforced ceramic Substances 0.000 title claims description 6
- 238000004519 manufacturing process Methods 0.000 title claims description 5
- 239000000835 fiber Substances 0.000 title 1
- 239000012783 reinforcing fiber Substances 0.000 claims description 27
- 239000004094 surface-active agent Substances 0.000 claims description 24
- 239000000919 ceramic Substances 0.000 claims description 14
- 239000003960 organic solvent Substances 0.000 claims description 13
- 239000000843 powder Substances 0.000 claims description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 12
- 238000002156 mixing Methods 0.000 claims description 10
- 238000005245 sintering Methods 0.000 claims description 3
- 239000011248 coating agent Substances 0.000 claims description 2
- 238000000576 coating method Methods 0.000 claims description 2
- 238000000034 method Methods 0.000 description 10
- 239000011159 matrix material Substances 0.000 description 7
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 7
- 239000000243 solution Substances 0.000 description 6
- 238000000465 moulding Methods 0.000 description 5
- 229910010271 silicon carbide Inorganic materials 0.000 description 5
- 229910052581 Si3N4 Inorganic materials 0.000 description 4
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 4
- 238000005452 bending Methods 0.000 description 3
- 238000007796 conventional method Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 239000002736 nonionic surfactant Substances 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 2
- 230000002776 aggregation Effects 0.000 description 2
- 239000011230 binding agent Substances 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 238000001746 injection moulding Methods 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 238000000967 suction filtration Methods 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 229910003460 diamond Inorganic materials 0.000 description 1
- 239000010432 diamond Substances 0.000 description 1
- KZHJGOXRZJKJNY-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Si]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O KZHJGOXRZJKJNY-UHFFFAOYSA-N 0.000 description 1
- 238000007580 dry-mixing Methods 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 238000007731 hot pressing Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000011812 mixed powder Substances 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 229910052863 mullite Inorganic materials 0.000 description 1
- 238000013001 point bending Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000007569 slipcasting Methods 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 238000002604 ultrasonography Methods 0.000 description 1
Landscapes
- Laminated Bodies (AREA)
Abstract
(57)【要約】本公報は電子出願前の出願データであるた
め要約のデータは記録されません。(57) [Summary] This bulletin contains application data before electronic filing, so abstract data is not recorded.
Description
【発明の詳細な説明】
（産業上の利用分野）
この発明は界面活性剤を用いることにより強化繊維のセ
ラミックマトリックスへの分散性を向上させた繊維強化
セラミックス複合材料の製造方法に関するものである。DETAILED DESCRIPTION OF THE INVENTION (Industrial Application Field) The present invention relates to a method for producing a fiber-reinforced ceramic composite material in which the dispersibility of reinforcing fibers in a ceramic matrix is improved by using a surfactant.
（従来の技術）
従来の繊維強化セラミックスの製造方法としては、例え
ば特開昭５９−５４６８０号公報に記載されている方法
がある。この方法ではセラミックス粉末として窒化ケイ
素粉末、強化繊維として炭化ケイ素（ＳｉＣ）ウィスカ
ーの如きＳｉＣ結晶を用い、それぞれを水および／また
は有機溶剤に分散させ、それぞれフィルターを通過させ
た後、それら分散液を混合し、次いで成形、焼結するこ
とにより繊維強化型窒化ケイ素焼結体を製造する。(Prior Art) As a conventional method for manufacturing fiber-reinforced ceramics, there is, for example, a method described in Japanese Patent Application Laid-Open No. 59-54680. In this method, silicon nitride powder is used as the ceramic powder, and SiC crystals such as silicon carbide (SiC) whiskers are used as the reinforcing fibers, each is dispersed in water and/or an organic solvent, and after each is passed through a filter, the dispersion is A fiber-reinforced silicon nitride sintered body is manufactured by mixing, then molding and sintering.
（発明が解決しようとする問題点）
しかしながら、このような従来の方法にあっては、Ｓｉ
Ｃウィスカーとセラミックス粉末とを混合する際予めＳ
ｉＣウィスカーおよびセラミックス粉末を夫々水および
／または有機溶剤中、超音波等により分散させ、フィル
ターを通過させろ過する。(Problem to be solved by the invention) However, in such a conventional method, Si
When mixing C whiskers and ceramic powder, S
The iC whiskers and ceramic powder are each dispersed in water and/or an organic solvent using ultrasonic waves, etc., and then passed through a filter and filtered.
しかしろ過したＳｉＣウィスカーとセラミックス粉末と
の混合液を乾燥する過程において、再度ＳｉＣウィスカ
ーの凝集が生じてしまうため、その混合物を原料とした
ＳｉＣウィスカー・セラミックス複合材料焼結体中には
ＳｉＣウィスカーの凝集塊が残存し、その焼結体の強度
等機械的性質に大きな影響を及ぼすばかりでなく、マト
リックス中へのＳｉＣウィスカーの均一な分散は望めず
、ウィスカー強化の効果が十分に発揮されないという問
題点があった。However, in the process of drying the filtered mixed solution of SiC whiskers and ceramic powder, the SiC whiskers agglomerate again. The problem is that agglomerates remain, which not only greatly affects the mechanical properties such as the strength of the sintered body, but also that uniform dispersion of SiC whiskers in the matrix cannot be expected, and the whisker strengthening effect is not fully demonstrated. There was a point.
（問題点を解決するための手段）
この発明は、水または有機溶剤に界面活性剤を添加し、
得られた溶液中に強化繊維を混合して強化繊維の表面を
界面活性剤で被覆すると強化繊維相互のからみ合いを減
することができることを知見したことに基づくものであ
る。(Means for solving the problem) This invention adds a surfactant to water or an organic solvent,
This is based on the finding that if reinforcing fibers are mixed into the obtained solution and the surfaces of the reinforcing fibers are coated with a surfactant, entanglement between the reinforcing fibers can be reduced.
従ってこの発明の繊維強化セラミックスの製造方法は、
水または有機溶剤の界面活性剤溶液中に強化繊維を混合
し、強化繊維表面を界面活性剤で被覆した後セラミック
ス粉末と混合し焼結することを特徴とする。Therefore, the method for manufacturing fiber-reinforced ceramics of this invention is as follows:
The method is characterized in that reinforcing fibers are mixed in a surfactant solution of water or an organic solvent, the surfaces of the reinforcing fibers are coated with the surfactant, and then mixed with ceramic powder and sintered.
この発明においては、先ず水または有機溶剤の界面活性
剤溶液中に強化繊維を混合する。強化繊維としてはＳｉ
Ｃウィスカー、窒化ケイ素（ＳｉＪ４）ウィスカー等の
セラミックウィスカーが好ましく用いられる。In this invention, first, reinforcing fibers are mixed into a surfactant solution of water or an organic solvent. Si as reinforcing fiber
Ceramic whiskers such as C whiskers and silicon nitride (SiJ4) whiskers are preferably used.
次に界面活性剤としては非イオン界面活性剤が好ましく
、なかでも次式
界面活性剤の分子量 ５
で表わされる親水性親油性バランス（ＨＬＢ）値が６．
０〜１６．０を示す非イオン界面活性剤が好ましく用い
られる。界面活性剤は、水または有機溶剤（好ましくは
水に近い極性を有する有機溶剤）に０．１容量％以上混
合した溶液とし、その溶液中に強化繊維を混合する。こ
の際、界面活性剤、溶媒、強化繊維の間の体積比を考慮
する必要があるが、強化繊維の体積に対し、５０倍以上
、好ましくは１００倍以上の界面活性剤溶液が適当であ
る。上記した以下の、あまりにも少ない量の界面活性剤
では、この発明の強化繊維を界面活性剤により被覆する
効果が得られない。また、ＨＬＢ値が１６．０を越える
界面活性剤では、水または有機溶媒中に溶解し、強化繊
維の表面を被覆する能力は無く、ＩＩＬＢ値が６．０未
満の界面活性剤は、水または有機溶媒、強化繊維、界面
活性剤の間で分離が生じ、同様に強化繊維表面を被覆す
ることはできない。強化繊維と、界面活性剤の水または
有機溶剤の混合液は、攪拌機や超音波照射等により十分
混合、分散した後、吸引ろ適法や乾燥器等により溶媒や
余剰の界面活性剤を除去する。こうして得られた界面活
性剤によりその表面を被覆した強化繊維は、相互のから
み合いが極めて少なく、また、乾燥過程において凝集を
形成したとしても容易に破壊することができる。また、
表面を界面活性剤で被覆した強化繊維は、次工程の、マ
トリックスとなるセラミックス粉末例えば窒化ケイ素、
炭化ケイ素、ジルコニア、ムライト、アルミナの粉体と
の混合過程においても容易に分散し、強化繊維だけの凝
集を形成することは非常に少ない。なお、マトリックス
との混合には、強化繊維を機械的に…傷させないことが
重要であり、■ブレンダーによる乾式混合、水または有
機溶剤中、成形用有機バインダー等を混合する湿式混合
、セラミックス射出成形に用いられるワックス、プラス
チック等の溶融物に機械的に混合する方法等が可能であ
る。Next, as the surfactant, nonionic surfactants are preferred, and among them, the hydrophilic-lipophilic balance (HLB) value expressed by the molecular weight of the surfactant of the following formula 5 is 6.
A nonionic surfactant having a molecular weight of 0 to 16.0 is preferably used. The surfactant is mixed into a solution of 0.1% by volume or more in water or an organic solvent (preferably an organic solvent having a polarity close to that of water), and the reinforcing fibers are mixed into the solution. At this time, it is necessary to consider the volume ratio between the surfactant, the solvent, and the reinforcing fibers, but it is appropriate to use a surfactant solution whose volume is at least 50 times, preferably at least 100 times, the volume of the reinforcing fibers. If the amount of the surfactant described below is too small, the effect of coating the reinforcing fibers of the present invention with the surfactant cannot be obtained. Additionally, surfactants with an HLB value of over 16.0 have no ability to dissolve in water or organic solvents and coat the surface of reinforcing fibers, and surfactants with an IILB value of less than 6.0 cannot be dissolved in water or organic solvents. Separation occurs between the organic solvent, the reinforcing fibers, and the surfactant, and the surface of the reinforcing fibers cannot be coated in the same way. A mixture of reinforcing fibers and a surfactant in water or an organic solvent is sufficiently mixed and dispersed using a stirrer or ultrasonic irradiation, and then the solvent and excess surfactant are removed using a suction filtration method, a dryer, or the like. The reinforcing fibers whose surfaces are coated with the surfactant thus obtained have very little mutual entanglement, and even if aggregates are formed during the drying process, they can be easily broken. Also,
The reinforcing fibers whose surfaces are coated with a surfactant are used in the next step to form a matrix of ceramic powder such as silicon nitride,
It is easily dispersed during the mixing process with silicon carbide, zirconia, mullite, and alumina powders, and there is very little chance of aggregation of reinforcing fibers alone. When mixing with the matrix, it is important not to mechanically damage the reinforcing fibers. ■Dry mixing using a blender, wet mixing in water or organic solvent, mixing an organic binder for molding, etc., and ceramic injection molding. Possible methods include mechanically mixing it into a melted material such as wax or plastic used for.
これらの方法により、セラミックス粉末と混合された原
料は、泥漿鋳込（スリップ・キャスト）、プレス成形、
射出成形等により所望の形状に成形した後、成形法によ
っては脱バインダーを行なった後、常法により焼結する
。By these methods, the raw materials mixed with ceramic powder are processed by slip casting, press molding,
After molding into a desired shape by injection molding or the like, the binder is removed depending on the molding method, and then sintering is performed by a conventional method.
（実施例） 次にこの発明を実施例および比較例により説明する。(Example) Next, the present invention will be explained with reference to Examples and Comparative Examples.
一施 １〜４．ｒｌ
表１に示すマトリックスとなる各セラミック粉末に、３
０容量％の炭化ケイ素（ＳｉＣ）ウィスカーを加え、１
００ｇとした。各混合粉末に、表示するＩＩＬＢを有す
る非イオン界面活性剤の２０容泄％水溶液を加え、全体
を１１とし、超音波を照射しつつ攪拌した。尚各原科の
特性を表２に示す。約１時量子分に混合した後、吸引ろ
適法により乾燥した。その後乾燥器内で十分乾燥した原
料をほぐし、この原料粉末を、黒鉛型を用いて真空中（
１０−２）ル（Ｔｏｒｒ）以下） 、３００ｋｇ／ｃが
の条件で４ＱｍｍＸ５ＱｌｌＸ約６ｆｌの形状にホット
プレス法により焼結した。Issei 1-4. rl For each ceramic powder serving as the matrix shown in Table 1, 3
Add 0% by volume of silicon carbide (SiC) whiskers,
00g. A 20% aqueous solution of a nonionic surfactant having the indicated IILB was added to each mixed powder to give a total volume of 11, and the mixture was stirred while being irradiated with ultrasound. The characteristics of each family are shown in Table 2. After mixing for about 1 hour, the mixture was dried by suction filtration. After that, the sufficiently dried raw material is loosened in a dryer, and this raw material powder is mixed in a vacuum using a graphite mold (
10-2) Torr or less) and 300 kg/c were sintered into a shape of 4Q mm x 5 Qll x about 6 fl by hot pressing.
ポットプレスの温度と保持時間は次の通りである。The temperature and holding time of the pot press are as follows.
得られた焼結体を厚さ約３１■に研削し、最終的に１１
４００のダイヤモンド砥石で仕上げた後、３１１×４ｍ
ｍＸ４０＋ｎに切り出し、実施例１〜４の抗折試験片と
した。The obtained sintered body was ground to a thickness of about 31 cm, and finally
After finishing with 400 diamond whetstone, 311 x 4m
It was cut out to m x 40+n and used as bending test pieces of Examples 1 to 4.
また比較のため界面活性剤を用いなかったこと以外は実
施例１と同様にして比較例１の焼結体を得、この焼結体
から同様にして抗折試験片を得た。For comparison, a sintered body of Comparative Example 1 was obtained in the same manner as in Example 1 except that no surfactant was used, and a bending test piece was obtained from this sintered body in the same manner.
上記各試験片につき研摩面および破面の観察を電子顕微
鏡（ＳＥＭ）を用いて行い、更にＪＩＳ Ｒ１６０１「
ファインセラミックスの曲げ強さ試験法」に従って３点
曲げ強さを測定し、試料５本の測定結果の平均値を、表
１に示す。The polished surface and fracture surface of each of the above specimens were observed using an electron microscope (SEM), and further JIS R1601 "
The three-point bending strength was measured according to the "Bending Strength Test Method for Fine Ceramics", and the average value of the measurement results of five samples is shown in Table 1.
表 １
表 ２
（発明の効果）
以上説明してきたように、この発明によれば、界面活性
剤でその表面を被覆した強化繊維を用いることにより、
マトリックスのセラミックス粉末との混合においても強
化繊維の凝集が形成されないため、強化繊維がマトリッ
クス中に均一に分散した繊維強化セラミックス複合材料
の焼結体が製造できるという効果かえられる。Table 1 Table 2 (Effects of the invention) As explained above, according to the present invention, by using reinforcing fibers whose surfaces are coated with a surfactant,
Since no agglomeration of the reinforcing fibers is formed when the reinforcing fibers are mixed with the ceramic powder of the matrix, it is possible to produce a sintered body of a fiber-reinforced ceramic composite material in which the reinforcing fibers are uniformly dispersed in the matrix.
Claims (1)
混合し、強化繊維表面を界面活性剤で被覆した後セラミ
ックス粉末と混合し、焼結することを特徴とする繊維強
化セラミックスの製造方法。1. A method for producing fiber-reinforced ceramics, which comprises mixing reinforcing fibers in a surfactant solution of water or an organic solvent, coating the surface of the reinforcing fibers with the surfactant, and then mixing with ceramic powder and sintering. .
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP61152891A JPS6311579A (en) | 1986-06-30 | 1986-06-30 | Manufacture of fiber reinforced ceramics |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP61152891A JPS6311579A (en) | 1986-06-30 | 1986-06-30 | Manufacture of fiber reinforced ceramics |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPS6311579A true JPS6311579A (en) | 1988-01-19 |
Family
ID=15550384
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP61152891A Pending JPS6311579A (en) | 1986-06-30 | 1986-06-30 | Manufacture of fiber reinforced ceramics |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS6311579A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH01278479A (en) * | 1988-04-28 | 1989-11-08 | Hitachi Metals Ltd | Whisker compound ceramic and production thereof |
-
1986
- 1986-06-30 JP JP61152891A patent/JPS6311579A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH01278479A (en) * | 1988-04-28 | 1989-11-08 | Hitachi Metals Ltd | Whisker compound ceramic and production thereof |
| JP2565981B2 (en) * | 1988-04-28 | 1996-12-18 | 日立金属株式会社 | Whisker composite ceramics and manufacturing method thereof |
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